CN114377559A - Super-hydrophobic nano-cellulose moisture-resistant air purification membrane and preparation method thereof - Google Patents
Super-hydrophobic nano-cellulose moisture-resistant air purification membrane and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a super-hydrophobic nano-cellulose humidity-resistant air purification membrane and a preparation method thereof, and the nano-cellulose air purification membrane with super-hydrophobic property is obtained, so that the nano-cellulose air purification membrane can be stably filtered under the high-humidity environment condition. The invention adopts a form of combining green chemical modification and freeze drying process, and the method has the advantages of safety, stability, simple production process and low process cost.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of air purification membranes, in particular to a super-hydrophobic nano-cellulose anti-humidity air purification membrane and a preparation method thereof.
[ background of the invention ]
Sustainable development is a basic concept of the current social development, and the adoption of plant source materials to replace non-renewable materials is imperative. Since the world is attacked by new coronavirus, the manufacturing of air filtering equipment has been rapidly increased, and a mask filter element is mainly used as a representative. The related data show that the productivity of the mask filter element is improved by nearly three times in 2020. At present, the mask filter element still uses petroleum derivative polypropylene as a main material source, the increase of the productivity inevitably increases the carbon emission, and meanwhile, the defect of incapability of natural degradation causes secondary pollution to the ecological environment.
Based on this, it has been studied to prepare a highly efficient air purification membrane using nanocellulose degradable by plant fiber as a substrate, and related studies have been made, for example, chinese patent application No. 201810717317.5, a cellulose-polyamide antistatic air purification composite membrane and a preparation method thereof, in which graphene oxide and tetra-carboxyl iron phthalocyanine are added to a cellulose/polyamide spinning emulsion, and the graphene oxide is precipitated and deposited on the surface of the composite nanomembrane by demulsification during solidification, and a layer of tetra-carboxyl iron phthalocyanine is further grafted on the surface, and the prepared composite membrane can fully utilize the catalytic oxidation capability of the tetra-carboxyl iron phthalocyanine on formaldehyde, and has a highly efficient and permanent removal effect on formaldehyde, and can remove static electricity in time, prevent dust adsorption, prevent membrane pore blocking, and has good durability and long service life, and can be widely used in the field of air purification. For example, Chinese patent application No. 201710587286.1 discloses a method for preparing negative ion air purification membrane, which comprises dissolving cellulose acetate as main material in single solvent or mixed solvent to obtain mixed fiber solution, mixing with modified tourmaline powder, homogenizing, and electrospinning to obtain novel negative ion air purification membrane with surface density of 30-120g/m2Thickness of 0.3-0.8mm, tensile strength: 8-15KN/M, the air purification membrane is prepared by taking cellulose acetate as a main component, the method is simple, and the mirabilite powder is added on the purification membrane to bring negative ions while filtering air, so that the aim of purifying air is achieved.
However, the plant fiber nano-cellulose is a hydrophilic fiber, and the basic characteristics of the material cause the limitation of the application in different scenes, especially in the environment of high humidity and high temperature difference, and are particularly represented by the following two points: 1. the plant fiber is easy to absorb moisture and swell under the high humidity environment, so that the fiber structure is softened, and finally, the fiber net structure collapses under the air pressure difference environment in the using process, so that the most basic filtering performance is lost; 2. the electrostatic spinning membrane of the electrostatic column electrode is interfered by water molecules in high-humidity air, so that the surface charge carried by the electrostatic spinning membrane is lost, and the filtration efficiency taking electrostatic adsorption force as the dominant factor is reduced. In practical environmental conditions, the Relative Humidity (RH) of air in tropical or subtropical regions can reach 80-90%, and human mouth and nose breath can generate aerosol humid hot air containing 85-95% RH. When a certain temperature difference exists between the two ends of the air purification membrane, the wet air flow can be condensed to form liquid drops when passing through the filter medium based on the condensation effect. The damage of the condensation phenomenon to the structure of the fiber filtering membrane is destructive, on one hand, the mechanical property is greatly reduced because the hydrophilic fiber absorbs liquid drops, and the stretching resistance and the bending resistance of the filtering membrane are insufficient; on the other hand, the capillary force causes the trapped liquid droplets to aggregate between the fibers to form a liquid film, so that the air flow path of the filter medium is reduced, resulting in an increase in filtration resistance.
Therefore, the insufficient moisture resistance of the nano-cellulose air purification membrane at present is a key factor limiting the application of the nano-cellulose air purification membrane.
[ summary of the invention ]
Aiming at the problem of insufficient humidity resistance of a nano-cellulose air purification membrane in the prior art, the invention provides a super-hydrophobic nano-cellulose humidity-resistant air purification membrane and a preparation method thereof, so that the nano-cellulose air purification membrane with super-hydrophobic property is obtained, and stable filtration of the nano-cellulose air purification membrane under a high-humidity environment condition is realized. The invention adopts a form of combining green chemical modification and freeze drying process, and the method has the advantages of safety, stability, simple production process and low process cost.
The purpose of the invention is realized by the following technical scheme:
the preparation method of the super-hydrophobic nano cellulose anti-humidity air purification membrane comprises the following steps:
1) preparing 40-60 parts of nano-cellulose, 0.1-1 part of methyltrimethoxysilane, 40-60 parts of tert-butyl alcohol and 2-4 parts of purified water by weight, uniformly mixing the nano-cellulose and the tert-butyl alcohol, and homogenizing under an ultrasonic condition;
2) adjusting the pH value of the purified water to 4, adding methyltrimethoxysilane, and uniformly stirring to prepare silane hydrolysate;
3) mixing the material obtained in the step 2) with the material obtained in the step 1), carrying out modification reaction under the stirring condition, shaping by using a customized die after the modification reaction is finished, freeze-drying, and annealing at high temperature to obtain the super-hydrophobic nano cellulose anti-humidity air purification membrane.
In the invention:
in the step 1), according to the weight ratio of 50 parts of nano-cellulose, 0.5 part of methyltrimethoxysilane, 50 parts of tert-butyl alcohol and 3 parts of purified water; the stirring is uniform, and magnetic stirring is adopted for 30 min; the ultrasonic condition is that the power is 100W and the time is 10 min.
The step 2) of uniformly stirring adopts magnetic stirring for 10 min.
The modification reaction is carried out under the stirring condition in the step 3), namely modification is carried out for 2 hours under the magnetic stirring condition; the molding is carried out by using a custom mold, wherein the size R of the mold is 6cm, and the height of the mold is 2 cm; the freeze drying is that the raw materials are firstly put into a refrigerator for pre-freezing for 6h at the temperature of minus 20 ℃ and then put into equipment for drying for 48h at the temperature of minus 56 ℃; and (3) annealing at the high temperature of 80 ℃ for 2 h.
The action and the effect of each component in the invention are as follows:
nano-cellulose: the supporting framework of the air purification membrane and the basic source of the filtering effect.
Methyltrimethoxysilane: the nano-cellulose hydrophobic modifier is used for realizing the super-hydrophobic performance of the nano-cellulose.
Tert-butyl alcohol: so that the nano-cellulose forms uniform and fine pores in the freeze drying process and the filtering performance is improved.
Hydrochloric acid: the condition of the pH value of the hydrolysis environment of the methyltrimethoxysilane leads the silane to be stably hydrolyzed.
The invention also relates to the super-hydrophobic nano-cellulose anti-moisture air purification membrane prepared by the preparation methodThe wet air purification membrane has the density of 0.0119-0.0153g/cm2The porosity reaches 99.0-99.2%, the water contact static angle reaches 138.5-154.2 degrees, the water contact rolling angle is 5.3-7.2 degrees, the filtration efficiency of PM2.5 reaches 99.24-99.73 percent, the filtration resistance is lower than 100Pa (51-82Pa), the quality factor reaches 0.076-0.122Pa-1And meets the requirement of commercial air filtering materials.
Compared with the prior art, the invention has the following advantages:
1. according to the preparation method of the super-hydrophobic nano-cellulose moisture-resistant air purification membrane, the nano-cellulose is modified in a chemical modification mode, the modification of methyltrimethoxysilane enhances the hydrophobic property of the nano-cellulose, the super-hydrophobic effect is achieved (the water contact static angle is 138.5-154.2 degrees, and the water contact rolling angle is 5.3-7.2 degrees), the anti-interference capability of the nano-cellulose air purification membrane on water in air is facilitated, the method is simple and effective in process, free of toxicity and harm, free of environmental pollution risk, low in production energy consumption, easy to realize industrialization, and the potential of industrial application of the nano-cellulose is further improved.
2. The super-hydrophobic nano-cellulose moisture-resistant air purification membrane obtained by the invention can obviously improve the moisture-resistant filtration performance of the nano-cellulose air purification membrane, ensure the high-efficiency particulate matter filtration efficiency and reduce the particulate matter filtration resistance, and compared with the existing product, the moisture-resistant performance is improved by about 50 times, and the moisture-resistant filtration resistance increase rate is lower than 15%. Meanwhile, the addition of the tertiary butanol keeps the highly uniform and fine pore structure of the nano-cellulose, and the density is 0.0119-0.0153g/cm2The porosity reaches 99.0-99.2%, the high-efficiency filtration performance of the nanofiber air purification membrane is realized, the filtration efficiency of PM2.5 reaches 99.24-99.73%, the filtration resistance is lower than 100Pa, and the quality factor reaches 0.076-0.122Pa-1And meets the requirement of commercial air filtering materials.
[ description of the drawings ]
Fig. 1 is a process flow chart of a preparation method of the super-hydrophobic nano cellulose anti-moisture air purification membrane of the invention.
[ detailed description ] embodiments
The following examples are provided to further illustrate the embodiments of the present invention.
Example 1:
the preparation method of the super-hydrophobic nano cellulose anti-humidity air purification membrane comprises the following steps:
1) preparing 50g of nano-cellulose, 0.5g of methyltrimethoxysilane, 50g of tert-butyl alcohol and 3g of purified water, uniformly mixing the nano-cellulose and the tert-butyl alcohol by adopting magnetic stirring for 30min, and homogenizing under the ultrasonic condition (power: 100W for 10 min);
2) adjusting the pH value of the purified water to be 4, adding methyltrimethoxysilane, and uniformly stirring (magnetically stirring for 10min) to prepare silane hydrolysate;
3) mixing the material obtained in the step 2) with the material obtained in the step 1), carrying out modification reaction for 2h under magnetic stirring, shaping by using a customized die (the size R of the die is 6cm, and the height of the die is 2cm) after the modification reaction is finished, freeze-drying (placing the die in a refrigerator for pre-freezing at-20 ℃ for 6h, then placing the die in a device at-56 ℃ for drying for 48h), and annealing at high temperature (the annealing temperature is 80 ℃ and the annealing time is 2h) to obtain the super-hydrophobic nano cellulose anti-humidity air purification membrane;
the obtained super-hydrophobic nano cellulose anti-humidity air purification membrane has the density of 0.0123g/cm2The porosity reaches 99.1%, the water contact static angle reaches 147.8 degrees, the water contact rolling angle is 6.4 degrees, the filtering efficiency of PM2.5 reaches 99.56 percent, the filtering resistance is 51Pa, and the quality factor reaches 0.107Pa-1。
Example 2:
the preparation method of the super-hydrophobic nano cellulose anti-humidity air purification membrane comprises the following steps:
1) preparing 40g of nano-cellulose, 1g of methyltrimethoxysilane, 40g of tert-butyl alcohol and 4g of purified water, uniformly mixing the nano-cellulose and the tert-butyl alcohol by adopting magnetic stirring for 30min, and homogenizing under the ultrasonic condition (power: 100W for 10 min);
2) adjusting the pH value of the purified water to be 4, adding methyltrimethoxysilane, and uniformly stirring (magnetically stirring for 10min) to prepare silane hydrolysate;
3) mixing the material obtained in the step 2) with the material obtained in the step 1), carrying out modification reaction for 2h under magnetic stirring, shaping by using a customized die (the size R of the die is 6cm, and the height of the die is 2cm) after the modification reaction is finished, freeze-drying (placing the die in a refrigerator for pre-freezing at-20 ℃ for 6h, then placing the die in a device at-56 ℃ for drying for 48h), and annealing at high temperature (the annealing temperature is 80 ℃ and the annealing time is 2h) to obtain the super-hydrophobic nano cellulose anti-humidity air purification membrane;
the obtained super-hydrophobic nano cellulose humidity-resistant air purification membrane has the density of 0.0151g/cm2The porosity reaches 99.0%, the water contact static angle reaches 154.2 degrees, the water contact rolling angle is 5.3 degrees, the filtering efficiency of PM2.5 reaches 99.73 percent, the filtering resistance is 82Pa, and the quality factor reaches 0.076Pa-1。
Example 3:
the preparation method of the super-hydrophobic nano cellulose anti-humidity air purification membrane comprises the following steps:
1) preparing 60g of nano-cellulose, 0.1g of methyltrimethoxysilane, 60g of tert-butyl alcohol and 2g of purified water, uniformly mixing the nano-cellulose and the tert-butyl alcohol by adopting magnetic stirring for 30min, and homogenizing under the ultrasonic condition (power: 100W for 10 min);
2) adjusting the pH value of the purified water to be 4, adding methyltrimethoxysilane, and uniformly stirring (magnetically stirring for 10min) to prepare silane hydrolysate;
3) mixing the material obtained in the step 2) with the material obtained in the step 1), carrying out modification reaction for 2h under magnetic stirring, shaping by using a customized die (the size R of the die is 6cm, and the height of the die is 2cm) after the modification reaction is finished, freeze-drying (placing the die in a refrigerator for pre-freezing at-20 ℃ for 6h, then placing the die in a device at-56 ℃ for drying for 48h), and annealing at high temperature (the annealing temperature is 80 ℃ and the annealing time is 2h) to obtain the super-hydrophobic nano cellulose anti-humidity air purification membrane;
the obtained super-hydrophobic nano cellulose anti-moisture air purification membrane has the density of 0.0119g/cm2The porosity reaches 99.2%, the water contact static angle reaches 138.5 degrees, the water contact rolling angle is 7.2 degrees, the filtering efficiency of PM2.5 reaches 99.24 percent, the filtering resistance is 52Pa, and the quality factor reaches 0.122Pa-1。
Example (c); and (3) screening:
TABLE 1 Material compounding table
The different technical schemes are as follows:
(1) placing 40% of nano cellulose in a beaker, adding 40% of tert-butanol, stirring for 30min under the action of magnetic stirring to mix uniformly, and then homogenizing by ultrasonic treatment (power: 30%, time 10 min). Preparing methyltrimethoxysilane separately, putting a proper amount of deionized water into a beaker, regulating the pH value of an aqueous solution to be 4 by hydrochloric acid, and then dropwise adding 1% methyltrimethoxysilane to hydrolyze for 10min under the action of magnetic stirring to obtain methyltrimethoxysilane hydrolysate for later use. Adding a proper amount of methyltrimethoxysilane hydrolysate into a nano-cellulose/tert-butyl alcohol mixed solution, modifying for 2h under the action of magnetic stirring, pouring into a customized mould (R is 6cm) after modification, pre-freezing for 6h in a refrigerator (20 ℃) and then freeze-drying (56 ℃ and 48h), taking out and sealing a freeze-dried sample, and annealing for 2h in a high-temperature oven at 80 ℃ to obtain the final sample.
(2) The difference with (1) lies in that the batching is than different, and corresponding batching is: 40% of nanocellulose and 50% of tert-butanol.
(3) The difference with (1) lies in that the batching is than different, and corresponding batching is: 40% of nanocellulose and 59% of tert-butanol.
(4) The difference with (1) lies in that the batching is than different, and corresponding batching is: 50% of nanocellulose and 40% of tert-butanol.
(5) The difference with (1) lies in that the batching is than different, and corresponding batching is: 50% of nanocellulose and 50% of tert-butanol.
(6) The difference with (1) lies in that the batching is than different, and corresponding batching is: 50% of nanocellulose and 59% of tert-butanol.
(7) The difference with (1) lies in that the batching is than different, and corresponding batching is: 60% of nanocellulose and 40% of tert-butanol.
(8) The difference with (1) lies in that the batching is than different, and corresponding batching is: 60% of nanocellulose and 50% of tert-butanol.
(9) The difference with (1) lies in that the batching is than different, and corresponding batching is: 60% of nanocellulose and 59% of tert-butanol.
The key technology of the invention is to investigate the influence effect of hydrophobic modification and anti-wet filtration of the nano-cellulose air purification membrane by different ingredient ratios, and construct the air purification membrane with different density and hydrophobic performance through the change of the ingredient ratio; the density of the air purification membrane is effectively reduced by increasing the proportion of the tert-butyl alcohol, the pore structure of the air purification membrane is further optimized, the specific surface area is increased, and the basic filtering effect of particles in different air environments is improved; the difference of nano-cellulose proportioning ratio mainly influences the hydrophobic property of the air purification membrane, the water contact angle of the air purification membrane is optimized to improve the water-resistant interference capacity of the air purification membrane, the problem that the filtration resistance is improved due to the fact that condensed wet air is effectively reduced, and the stable filtration effect of the nano-cellulose air purification membrane under high-humidity air can be achieved.
The above embodiments are only for illustrating the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention accordingly, and not to limit the protection scope of the present invention accordingly. All equivalent changes or modifications made in accordance with the spirit of the present disclosure are intended to be covered by the scope of the present disclosure.
Claims (9)
1. The preparation method of the super-hydrophobic nano cellulose anti-humidity air purification membrane is characterized by comprising the following steps: the method comprises the following steps:
1) preparing 40-60 parts of nano-cellulose, 0.1-1 part of methyltrimethoxysilane, 40-60 parts of tert-butyl alcohol and 2-4 parts of purified water by weight, uniformly mixing the nano-cellulose and the tert-butyl alcohol, and homogenizing under an ultrasonic condition;
2) adjusting the pH value of the purified water to 4, adding methyltrimethoxysilane, and uniformly stirring to prepare silane hydrolysate;
3) mixing the material obtained in the step 2) with the material obtained in the step 1), carrying out modification reaction under the stirring condition, shaping by using a customized die after the modification reaction is finished, freeze-drying, and annealing at high temperature to obtain the super-hydrophobic nano cellulose anti-humidity air purification membrane.
2. The preparation method of the superhydrophobic nanocellulose anti-moisture air purification membrane of claim 1, wherein: in the step 1), the weight ratio of 50 parts of nano-cellulose, 0.5 part of methyltrimethoxysilane, 50 parts of tertiary butanol and 3 parts of purified water is adopted.
3. The preparation method of the superhydrophobic nanocellulose anti-moisture air purification membrane of claim 1, wherein: the step 1) of uniformly stirring adopts magnetic stirring for 30 min.
4. The preparation method of the superhydrophobic nanocellulose anti-moisture air purification membrane of claim 1, wherein: the ultrasonic condition in the step 1) is that the power is 100W and the time is 10 min.
5. The preparation method of the superhydrophobic nanocellulose anti-moisture air purification membrane of claim 1, wherein: the step 2) of uniformly stirring adopts magnetic stirring for 10 min.
6. The preparation method of the superhydrophobic nanocellulose anti-moisture air purification membrane of claim 1, wherein: the modification reaction in the step 3) is carried out under the condition of stirring, and the modification is carried out for 2 hours under the condition of magnetic stirring.
7. The preparation method of the superhydrophobic nanocellulose anti-moisture air purification membrane of claim 1, wherein: shaping by using a custom mould in the step 3), wherein the size R of the mould is 6cm, and the height is 2 cm.
8. The preparation method of the superhydrophobic nanocellulose anti-moisture air purification membrane of claim 1, wherein: the freeze drying in the step 3) is to place the mixture in a refrigerator for pre-freezing for 6h at the temperature of minus 20 ℃ and then place the mixture in a device for drying for 48h at the temperature of minus 56 ℃; and (3) annealing at the high temperature of 80 ℃ for 2 h.
9. Super hydrophobic nanometer cellulose anti-humidity air purification membrane which characterized in that: the super-hydrophobic nano cellulose anti-moisture air purification membrane is prepared by the method of any one of claims 1 to 8.
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